#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/38/7103896.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7103896
loop_
_publ_author_name
'Cotton, F. Albert'
'Liu, Chun Y.'
'Murillo, Carlos A.'
'Wang, Xiaoping'
_publ_section_title
;
 A mixed-valence compound with one unpaired electron delocalized over four
 molybdenum atoms in a cyclic tetranuclear ion
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   17
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2190
_journal_page_last               2191
_journal_paper_doi               10.1039/b306822f
_journal_year                    2003
_chemical_formula_moiety         '[Mo2(C15H15N2O2)2]2Cl4(PF6)'
_chemical_formula_sum            'C60 H60 Cl4 F6 Mo4 N8 O8 P'
_chemical_formula_weight         1691.69
_chemical_name_common            (Mo2(DAniF)2)2Cl4(PF6)
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.1150(10)
_cell_angle_beta                 68.2310(10)
_cell_angle_gamma                67.4780(10)
_cell_formula_units_Z            1
_cell_length_a                   10.8175(8)
_cell_length_b                   13.0151(10)
_cell_length_c                   14.2603(10)
_cell_measurement_reflns_used    4948
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.008
_cell_measurement_theta_min      2.1705
_cell_volume                     1667.7(2)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'BRUKER-SMART 1000'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9524
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.75
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.994
_exptl_absorpt_correction_T_max  0.8197
_exptl_absorpt_correction_T_min  0.7022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.684
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             845
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0292P)²+0.8572P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0591
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                5660
_reflns_number_total             6432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306822f.txt
_cod_data_source_block           cmpd2
_cod_database_code               7103896
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.012150(19) 0.479840(16) 0.141927(14) 0.02207(6) Uani 1 1 d . . .
Mo2 Mo -0.115288(19) 0.633714(16) 0.063168(14) 0.02259(6) Uani 1 1 d . . .
P P 0.5000 0.0000 0.5000 0.0483(3) Uani 1 2 d S . .
F3 F 0.6361(2) 0.02205(18) 0.49985(15) 0.0663(5) Uani 1 1 d . . .
F1 F 0.4040(2) 0.10690(16) 0.54990(14) 0.0641(5) Uani 1 1 d . . .
F2 F 0.5071(2) 0.08310(16) 0.38605(13) 0.0668(5) Uani 1 1 d . . .
Cl1 Cl -0.03702(6) 0.32066(5) 0.11741(4) 0.02902(13) Uani 1 1 d . . .
Cl2 Cl 0.23880(6) 0.43350(5) 0.01061(4) 0.02956(13) Uani 1 1 d . . .
N1 N -0.14569(19) 0.47625(16) 0.28185(14) 0.0248(4) Uani 1 1 d . . .
N2 N -0.28031(19) 0.63995(16) 0.19678(14) 0.0254(4) Uani 1 1 d . . .
N3 N 0.09670(19) 0.57282(16) 0.18187(14) 0.0250(4) Uani 1 1 d . . .
N4 N -0.0468(2) 0.73672(16) 0.10419(14) 0.0253(4) Uani 1 1 d . . .
O1 O -0.0555(3) 0.17039(18) 0.65883(15) 0.0580(6) Uani 1 1 d . . .
O2 O -0.6942(2) 1.05998(18) 0.17569(18) 0.0574(6) Uani 1 1 d . . .
O3 O 0.5605(2) 0.39588(18) 0.33849(17) 0.0512(5) Uani 1 1 d . . .
O4 O -0.2990(2) 1.21017(15) 0.03720(15) 0.0455(5) Uani 1 1 d . . .
C10 C -0.2645(2) 0.5593(2) 0.28355(18) 0.0268(5) Uani 1 1 d . . .
H10A H -0.3361 0.5611 0.3450 0.032 Uiso 1 1 calc R . .
C11 C -0.1253(2) 0.3958(2) 0.37829(18) 0.0270(5) Uani 1 1 d . . .
C12 C -0.0669(3) 0.2806(2) 0.38452(19) 0.0349(6) Uani 1 1 d . . .
H12A H -0.0439 0.2543 0.3258 0.042 Uiso 1 1 calc R . .
C13 C -0.0410(3) 0.2014(2) 0.4767(2) 0.0390(6) Uani 1 1 d . . .
H13A H -0.0005 0.1237 0.4789 0.047 Uiso 1 1 calc R . .
C14 C -0.0759(3) 0.2396(2) 0.5644(2) 0.0400(6) Uani 1 1 d . . .
C15 C -0.1340(4) 0.3561(3) 0.5581(2) 0.0634(10) Uani 1 1 d . . .
H15A H -0.1581 0.3825 0.6169 0.076 Uiso 1 1 calc R . .
C16 C -0.1569(3) 0.4337(2) 0.4663(2) 0.0508(8) Uani 1 1 d . . .
H16A H -0.1938 0.5117 0.4633 0.061 Uiso 1 1 calc R . .
C17 C 0.0020(4) 0.0508(3) 0.6677(2) 0.0606(9) Uani 1 1 d . . .
H17A H 0.0115 0.0121 0.7370 0.091 Uiso 1 1 calc R . .
H17B H 0.0916 0.0361 0.6183 0.091 Uiso 1 1 calc R . .
H17C H -0.0583 0.0230 0.6539 0.091 Uiso 1 1 calc R . .
C21 C -0.3958(2) 0.7417(2) 0.19948(18) 0.0276(5) Uani 1 1 d . . .
C22 C -0.4456(3) 0.7948(2) 0.2800(2) 0.0374(6) Uani 1 1 d . . .
H22A H -0.4102 0.7598 0.3377 0.045 Uiso 1 1 calc R . .
C23 C -0.5478(3) 0.8996(3) 0.2757(2) 0.0453(7) Uani 1 1 d . . .
H23A H -0.5822 0.9335 0.3313 0.054 Uiso 1 1 calc R . .
C24 C -0.5984(3) 0.9539(2) 0.1892(2) 0.0396(6) Uani 1 1 d . . .
C25 C -0.5507(3) 0.9006(2) 0.1091(2) 0.0381(6) Uani 1 1 d . . .
H25A H -0.5867 0.9355 0.0517 0.046 Uiso 1 1 calc R . .
C26 C -0.4502(3) 0.7959(2) 0.1138(2) 0.0337(6) Uani 1 1 d . . .
H26A H -0.4183 0.7611 0.0591 0.040 Uiso 1 1 calc R . .
C27 C -0.7152(4) 1.1294(3) 0.2396(3) 0.0713(11) Uani 1 1 d . . .
H27A H -0.7836 1.2012 0.2225 0.107 Uiso 1 1 calc R . .
H27B H -0.6293 1.1434 0.2285 0.107 Uiso 1 1 calc R . .
H27C H -0.7472 1.0911 0.3114 0.107 Uiso 1 1 calc R . .
C30 C 0.0483(2) 0.68660(19) 0.15664(17) 0.0261(5) Uani 1 1 d . . .
H30A H 0.0809 0.7307 0.1757 0.031 Uiso 1 1 calc R . .
C31 C 0.2173(2) 0.52301(19) 0.22134(17) 0.0251(5) Uani 1 1 d . . .
C32 C 0.2284(2) 0.4233(2) 0.30121(19) 0.0291(5) Uani 1 1 d . A .
H32A H 0.1589 0.3871 0.3277 0.035 Uiso 1 1 calc R . .
C33 C 0.3424(2) 0.3769(2) 0.34220(19) 0.0317(5) Uani 1 1 d . . .
H33A H 0.3490 0.3100 0.3958 0.038 Uiso 1 1 calc R A .
C34 C 0.4457(3) 0.4309(2) 0.3027(2) 0.0323(5) Uani 1 1 d . A .
C35 C 0.4376(3) 0.5279(2) 0.2197(2) 0.0363(6) Uani 1 1 d . . .
H35A H 0.5088 0.5625 0.1915 0.044 Uiso 1 1 calc R A .
C36 C 0.3256(3) 0.5732(2) 0.17886(19) 0.0328(5) Uani 1 1 d . A .
H36A H 0.3220 0.6375 0.1227 0.039 Uiso 1 1 calc R . .
C37A C 0.537(3) 0.327(3) 0.448(3) 0.036(7) Uani 0.18(3) 1 d P A 1
H37A H 0.4855 0.3773 0.4936 0.054 Uiso 0.18(3) 1 calc PR A 1
H37B H 0.6248 0.2827 0.4624 0.054 Uiso 0.18(3) 1 calc PR A 1
H37C H 0.4851 0.2763 0.4583 0.054 Uiso 0.18(3) 1 calc PR A 1
C37B C 0.5771(13) 0.2972(12) 0.4208(12) 0.077(3) Uani 0.82(3) 1 d P A 2
H37D H 0.6289 0.2309 0.3932 0.115 Uiso 0.82(3) 1 calc PR A 2
H37E H 0.4874 0.2893 0.4645 0.115 Uiso 0.82(3) 1 calc PR A 2
H37F H 0.6265 0.3037 0.4612 0.115 Uiso 0.82(3) 1 calc PR A 2
C41 C -0.1107(2) 0.85854(19) 0.08975(18) 0.0251(5) Uani 1 1 d . . .
C42 C -0.1734(3) 0.9074(2) 0.17389(19) 0.0315(5) Uani 1 1 d . . .
H42A H -0.1727 0.8609 0.2407 0.038 Uiso 1 1 calc R . .
C43 C -0.2374(3) 1.0247(2) 0.1603(2) 0.0347(6) Uani 1 1 d . . .
H43A H -0.2791 1.0566 0.2174 0.042 Uiso 1 1 calc R . .
C44 C -0.2385(3) 1.0937(2) 0.0609(2) 0.0313(5) Uani 1 1 d . . .
C45 C -0.1762(3) 1.0452(2) -0.02395(19) 0.0307(5) Uani 1 1 d . . .
H45A H -0.1764 1.0918 -0.0908 0.037 Uiso 1 1 calc R . .
C46 C -0.1141(2) 0.9285(2) -0.00962(18) 0.0276(5) Uani 1 1 d . . .
H46A H -0.0744 0.8965 -0.0666 0.033 Uiso 1 1 calc R . .
C47 C -0.3659(3) 1.2659(2) 0.1210(2) 0.0543(8) Uani 1 1 d . . .
H47A H -0.4031 1.3468 0.0936 0.081 Uiso 1 1 calc R . .
H47B H -0.2995 1.2537 0.1565 0.081 Uiso 1 1 calc R . .
H47C H -0.4400 1.2345 0.1691 0.081 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Mo1 N1 91.60(7) . . y
N3 Mo1 Mo2 92.11(5) . . y
N1 Mo1 Mo2 91.68(5) . . y
N3 Mo1 Cl2 86.41(5) . . y
N1 Mo1 Cl2 162.50(5) . . y
Mo2 Mo1 Cl2 105.757(17) . . y
N3 Mo1 Cl1 163.08(5) . . y
N1 Mo1 Cl1 89.65(5) . . y
Mo2 Mo1 Cl1 104.721(17) . . y
Cl2 Mo1 Cl1 87.33(2) . . y
N2 Mo2 N4 89.06(7) . . y
N2 Mo2 Mo1 92.17(5) . . y
N4 Mo2 Mo1 91.80(5) . . y
N2 Mo2 Cl1 163.55(5) . 2_565 y
N4 Mo2 Cl1 89.25(5) . 2_565 y
Mo1 Mo2 Cl1 104.232(17) . 2_565 y
N2 Mo2 Cl2 90.07(5) . 2_565 y
N4 Mo2 Cl2 163.05(5) . 2_565 y
Mo1 Mo2 Cl2 105.152(17) . 2_565 y
Cl1 Mo2 Cl2 86.82(2) 2_565 2_565 y
F2 P F2 180.00(9) 2_656 . ?
F2 P F3 89.81(11) 2_656 . ?
F2 P F3 90.19(11) . . ?
F2 P F3 90.19(11) 2_656 2_656 ?
F2 P F3 89.81(11) . 2_656 ?
F3 P F3 180.00(14) . 2_656 ?
F2 P F1 89.86(10) 2_656 . ?
F2 P F1 90.14(10) . . ?
F3 P F1 89.98(10) . . ?
F3 P F1 90.02(10) 2_656 . ?
F2 P F1 90.14(10) 2_656 2_656 ?
F2 P F1 89.86(10) . 2_656 ?
F3 P F1 90.02(10) . 2_656 ?
F3 P F1 89.98(10) 2_656 2_656 ?
F1 P F1 180.00(12) . 2_656 ?
Mo1 Cl1 Mo2 85.262(19) . 2_565 ?
Mo1 Cl2 Mo2 85.287(19) . 2_565 ?
C10 N1 C11 118.58(19) . . ?
C10 N1 Mo1 118.27(15) . . ?
C11 N1 Mo1 122.75(15) . . ?
C10 N2 C21 120.7(2) . . ?
C10 N2 Mo2 118.59(16) . . ?
C21 N2 Mo2 119.45(15) . . ?
C30 N3 C31 117.35(19) . . ?
C30 N3 Mo1 117.92(15) . . ?
C31 N3 Mo1 124.10(14) . . ?
C30 N4 C41 118.27(18) . . ?
C30 N4 Mo2 118.60(15) . . ?
C41 N4 Mo2 122.65(14) . . ?
C14 O1 C17 117.6(2) . . ?
C24 O2 C27 117.2(2) . . ?
C34 O3 C37B 118.5(4) . . ?
C34 O3 C37A 112.0(13) . . ?
C44 O4 C47 118.1(2) . . ?
N1 C10 N2 119.3(2) . . ?
C12 C11 C16 118.3(2) . . ?
C12 C11 N1 121.0(2) . . ?
C16 C11 N1 120.6(2) . . ?
C11 C12 C13 121.8(2) . . ?
C14 C13 C12 119.4(2) . . ?
O1 C14 C13 124.7(2) . . ?
O1 C14 C15 116.5(2) . . ?
C13 C14 C15 118.8(2) . . ?
C16 C15 C14 121.3(3) . . ?
C15 C16 C11 120.3(3) . . ?
C22 C21 C26 118.5(2) . . ?
C22 C21 N2 121.7(2) . . ?
C26 C21 N2 119.4(2) . . ?
C21 C22 C23 120.8(2) . . ?
C24 C23 C22 120.2(2) . . ?
O2 C24 C23 124.4(2) . . ?
O2 C24 C25 116.2(2) . . ?
C23 C24 C25 119.4(2) . . ?
C26 C25 C24 120.4(2) . . ?
C25 C26 C21 120.7(2) . . ?
N4 C30 N3 119.4(2) . . ?
C32 C31 C36 119.0(2) . . ?
C32 C31 N3 120.4(2) . . ?
C36 C31 N3 120.6(2) . . ?
C31 C32 C33 120.8(2) . . ?
C34 C33 C32 119.5(2) . . ?
O3 C34 C33 125.1(2) . . ?
O3 C34 C35 115.2(2) . . ?
C33 C34 C35 119.7(2) . . ?
C36 C35 C34 120.7(2) . . ?
C35 C36 C31 120.2(2) . . ?
C42 C41 C46 119.0(2) . . ?
C42 C41 N4 121.0(2) . . ?
C46 C41 N4 119.9(2) . . ?
C41 C42 C43 121.1(2) . . ?
C44 C43 C42 119.4(2) . . ?
O4 C44 C43 125.1(2) . . ?
O4 C44 C45 115.1(2) . . ?
C43 C44 C45 119.9(2) . . ?
C46 C45 C44 120.4(2) . . ?
C45 C46 C41 120.2(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 N3 2.0860(18) . y
Mo1 N1 2.0897(19) . y
Mo1 Mo2 2.1453(3) . y
Mo1 Cl2 2.4796(6) . y
Mo1 Cl1 2.4891(6) . y
Mo2 N2 2.0736(19) . y
Mo2 N4 2.0809(18) . y
Mo2 Cl1 2.4921(6) 2_565 y
Mo2 Cl2 2.5003(6) 2_565 y
P F2 1.5919(18) 2_656 ?
P F3 1.603(2) 2_656 ?
P F1 1.6036(17) 2_656 ?
N1 C10 1.324(3) . ?
N1 C11 1.435(3) . ?
N2 C10 1.325(3) . ?
N2 C21 1.431(3) . ?
N3 C30 1.328(3) . ?
N3 C31 1.441(3) . ?
N4 C30 1.323(3) . ?
N4 C41 1.438(3) . ?
O1 C14 1.371(3) . ?
O1 C17 1.415(4) . ?
O2 C24 1.371(3) . ?
O2 C27 1.405(4) . ?
O3 C34 1.371(3) . ?
O3 C37B 1.402(10) . ?
O3 C37A 1.48(4) . ?
O4 C44 1.371(3) . ?
O4 C47 1.432(3) . ?
C11 C12 1.369(3) . ?
C11 C16 1.389(3) . ?
C12 C13 1.398(3) . ?
C13 C14 1.379(4) . ?
C14 C15 1.383(4) . ?
C15 C16 1.378(4) . ?
C21 C22 1.381(3) . ?
C21 C26 1.392(3) . ?
C22 C23 1.386(4) . ?
C23 C24 1.380(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.377(4) . ?
C31 C32 1.387(3) . ?
C31 C36 1.394(3) . ?
C32 C33 1.392(3) . ?
C33 C34 1.384(3) . ?
C34 C35 1.388(4) . ?
C35 C36 1.374(3) . ?
C41 C42 1.383(3) . ?
C41 C46 1.390(3) . ?
C42 C43 1.388(3) . ?
C43 C44 1.382(3) . ?
C44 C45 1.390(3) . ?
C45 C46 1.378(3) . ?
